CN111974656A - Super-hydrophobic coating and preparation method thereof - Google Patents
Super-hydrophobic coating and preparation method thereof Download PDFInfo
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- CN111974656A CN111974656A CN202010881988.2A CN202010881988A CN111974656A CN 111974656 A CN111974656 A CN 111974656A CN 202010881988 A CN202010881988 A CN 202010881988A CN 111974656 A CN111974656 A CN 111974656A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
- B05D5/08—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain an anti-friction or anti-adhesive surface
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/24—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials for applying particular liquids or other fluent materials
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F222/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a carboxyl radical and containing at least one other carboxyl radical in the molecule; Salts, anhydrides, esters, amides, imides, or nitriles thereof
- C08F222/10—Esters
- C08F222/1006—Esters of polyhydric alcohols or polyhydric phenols
- C08F222/103—Esters of polyhydric alcohols or polyhydric phenols of trialcohols, e.g. trimethylolpropane tri(meth)acrylate
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D135/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a carboxyl radical, and containing at least another carboxyl radical in the molecule, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Coating compositions based on derivatives of such polymers
- C09D135/02—Homopolymers or copolymers of esters
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2502/00—Acrylic polymers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2503/00—Polyurethanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- Life Sciences & Earth Sciences (AREA)
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- Polymers & Plastics (AREA)
- Medicinal Chemistry (AREA)
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Abstract
The invention provides a preparation method of a super-hydrophobic coating, which comprises the following steps: (1) adding ethyl acetate, methyl methacrylate, trimethylolpropane trimethacrylate and azobisisobutyronitrile into a reaction container to react to prepare a cross-linked polymethyl methacrylate solution; (2) mixing the crosslinked polymethyl methacrylate solution with the polyurethane adhesive, and uniformly stirring to form a spray colloidal suspension; (3) spraying the spray colloid suspension on the surface of the base material in a cold spraying mode; (4) and spraying the fluorinated nano-particles on the surface of the base material in a cold spraying mode to prepare the super-hydrophobic coating. The method comprises the steps of forming a colloidal suspension with an interpenetrating network structure by using a cross-linked polymethyl methacrylate solution and a polyurethane adhesive, coating the colloidal suspension on the surface of a base material by adopting cold spraying, solidifying the colloidal suspension to form a groove structure, and spraying fluorinated nano-particles on the surface of the base material to obtain the super-hydrophobic coating with excellent wear resistance and aging resistance.
Description
Technical Field
The invention relates to the technical field of preparation of novel coatings, in particular to a super-hydrophobic coating and a preparation method thereof.
Background
The preparation method of the super-hydrophobic coating is various, and the process is mature day by day, such as an ATRP method, a casting method, a chemical vapor deposition method, an electrospinning method, an etching method, a spraying method and the like. The preparation work of the super-hydrophobic coating has been greatly advanced, a plurality of preparation methods are continuously available, and the treatment of pollutants in industrial production has also been achieved with considerable results. The method protects the ecological environment to a certain extent, improves the industrial production benefit, reduces the consumption of raw materials and energy, and brings great benefits to production life. The preparation and application of the super-hydrophobic material reach a rather mature height at present, but still have some problems which are not solved yet. For example, the raw materials are expensive, the mechanical durability is poor, the structure is dependent, the aging is easy, the service life is short, the cost is high, and the industrialization is difficult. Therefore, for scientific research workers, research on the super-hydrophobic material still needs more energy and time to find a more efficient and economic preparation method, and the research is hard to overcome and the product which meets the requirements of people is developed.
Therefore, it is necessary to provide an abrasion-resistant and aging-resistant superhydrophobic coating and a preparation method thereof to solve the above technical problems.
Disclosure of Invention
The invention aims to provide a preparation method of a super-hydrophobic coating, and the super-hydrophobic coating prepared by the method has good wear resistance and aging resistance.
The invention also aims to provide a super-hydrophobic coating which is prepared by adopting the method.
In order to achieve the above object, the present invention provides a method for preparing a superhydrophobic coating, comprising the steps of:
(1) adding ethyl acetate, Methyl Methacrylate (MMA), trimethylolpropane trimethacrylate (TMPTMA) and Azobisisobutyronitrile (AIBN) into a reaction container for reaction to prepare a cross-linked polymethyl methacrylate solution;
(2) mixing the crosslinked polymethyl methacrylate solution with the polyurethane adhesive, and uniformly stirring to form a spray colloidal suspension;
(3) spraying the spraying colloid suspension on the surface of the base material, and curing at room temperature;
(4) and (4) spraying the fluorinated nano-particles on the surface of the base material on the basis of the step (3), curing at room temperature, and preparing the super-hydrophobic coating on the surface of the base material.
Compared with the prior art, the preparation method of the super-hydrophobic coating has the advantages that ethyl acetate, Methyl Methacrylate (MMA), trimethylolpropane trimethacrylate (TMPTMA) and Azobisisobutyronitrile (AIBN) are reacted to prepare a cross-linked polymethyl methacrylate solution, then the cross-linked polymethyl methacrylate solution and a polyurethane adhesive are utilized to form a colloidal suspension with an interpenetrating network structure, then the colloidal suspension is uniformly coated on the surface of a base material by adopting a cold spraying method, a groove structure is formed by solidification, the friction resistance of the coating is effectively improved, and finally, fluorinated nano-particles are sprayed on the surface of the base material, so that the aging resistance of the coating is greatly improved, and the super-hydrophobic coating is prepared. Therefore, the super-hydrophobic coating has excellent wear resistance and aging resistance.
Further, in the step (1), 30 to 70 parts of ethyl acetate, 10 to 50 parts of Methyl Methacrylate (MMA), 5 to 40 parts of trimethylolpropane trimethacrylate (TMPTMA) and 1 to 20 parts of Azobisisobutyronitrile (AIBN) are added.
Further, in the step (1), the reaction temperature is 50-80 ℃.
Further, in the step (1), the reaction time is 12-36 h.
Further, in the step (1), oil bath heating is adopted.
Further, in the step (2), 40-90 parts of crosslinked polymethyl methacrylate solution and 10-60 parts of polyurethane adhesive are added.
Further, in the step (2), mechanically stirring for 1-4 h.
Further, in the step (3), high-pressure gas of an air compressor is adopted for spraying.
Further, the fluorinated nanoparticles are selected from aluminum fluoride nanoparticles.
Correspondingly, the application also provides a super-hydrophobic coating, and the super-hydrophobic coating is prepared by adopting the preparation method of the super-hydrophobic coating.
Drawings
FIG. 1 is an SEM image of a cured superhydrophobic coating prepared in examples 1-4 of the present application, wherein FIGS. 1(a) - (d) correspond to examples 1-4, respectively.
Fig. 2 is an SEM image of the superhydrophobic coating prepared in example 4 of the present application after curing, and fig. 2(a) - (d) are SEM images of the superhydrophobic surface at different magnifications, respectively.
Detailed Description
The technical solutions of the present invention are further illustrated by the following specific embodiments, but the present invention is not limited thereto.
The sources of materials referred to in the examples are as follows:
example 1
A preparation method of a super-hydrophobic coating comprises the following steps:
(1) firstly, the stirring paddle is inserted into the three-mouth bottle, the blade is opened by rotation, then the three-mouth bottle is placed in the oil bath pot, the three-mouth bottle is fixed at a proper position of an iron support, the stirring paddle is connected with the stirring machine, and the experimental device is assembled. 60 parts of ethyl acetate are then added to a three-necked flask, followed by 30 parts of Methyl Methacrylate (MMA), 40 parts of trimethylolpropane trimethacrylate and 5 parts of Azobisisobutyronitrile (AIBN), the temperature of the oil bath being set at 60 ℃ and the reaction time being 18 h.
(2) Mixing 40% of cross-linked polymethyl methacrylate solution with 60% of polyurethane adhesive, and mechanically stirring for 2 hours to form spray colloidal suspension;
(3) uniformly spraying the spray colloidal suspension on the surface of the substrate by using high-pressure gas of an air compressor, and curing at room temperature for 30 min;
(4) and (4) after the coating in the step (3) is cured, spraying the aluminum fluoride nanoparticles on the surface of the base material by adopting high-pressure gas of an air compressor, curing at room temperature for 10min, and preparing the super-hydrophobic coating on the surface of the base material.
Examples 2 to 4
Examples 2 to 4 are substantially the same as example 1 except that the amounts of the crosslinked polymethylmethacrylate solution and the polyurethane binder used in step (2) of examples 2 to 4 are different as follows:
in example 2, step (2) a 60% crosslinked polymethylmethacrylate solution was mixed with 40% polyurethane binder and mechanically stirred for 2h to form a spray colloidal suspension;
in example 3, step (2) 80% cross-linked polymethylmethacrylate solution and 20% polyurethane binder were mixed and mechanically stirred for 2h to form a spray colloidal suspension;
in example 4, step (2) a 90% crosslinked polymethylmethacrylate solution was mixed with 10% polyurethane binder and mechanically stirred for 2h to form a spray colloidal suspension;
the rest is the same as example 1 and is not described here.
Examples 5 to 7
Examples 5 to 7 are substantially the same as example 1 except that the room temperature curing in step (4) of examples 5 to 7 is different as follows:
in the embodiment 5, (4) after the coating in the step (3) is cured, spraying the aluminum fluoride nanoparticles on the surface of the substrate by using high-pressure gas of an air compressor, and curing at room temperature for 20min to obtain a super-hydrophobic coating on the surface of the substrate;
in the embodiment 6, (4) after the coating in the step (3) is cured, spraying the aluminum fluoride nanoparticles on the surface of the substrate by using high-pressure gas of an air compressor, and curing at room temperature for 30min to obtain a super-hydrophobic coating on the surface of the substrate;
in the embodiment 7, (4) after the coating in the step (3) is cured, spraying the aluminum fluoride nanoparticles on the surface of the substrate by using high-pressure gas of an air compressor, and curing at room temperature for 40min to obtain a super-hydrophobic coating on the surface of the substrate;
the rest is the same as example 1 and is not described here.
Comparative example 1
A preparation method of a super-hydrophobic coating comprises the following steps:
(1) firstly, the stirring paddle is inserted into the three-mouth bottle, the blade is opened by rotation, then the three-mouth bottle is placed in the oil bath pot, the three-mouth bottle is fixed at a proper position of an iron support, the stirring paddle is connected with the stirring machine, and the experimental device is assembled. 60 parts of ethyl acetate are then added to a three-necked flask, followed by 30 parts of Methyl Methacrylate (MMA), 40 parts of trimethylolpropane trimethacrylate and 5 parts of Azobisisobutyronitrile (AIBN), the temperature of the oil bath being set at 60 ℃ and the reaction time being 18 h.
(2) Mixing 40% of cross-linked polymethyl methacrylate solution with 60% of polyurethane adhesive, and mechanically stirring for 2 hours to form spray colloidal suspension;
(3) and uniformly spraying the spray colloidal suspension on the surface of the substrate by adopting high-pressure gas of an air compressor, curing at room temperature for 30min, and preparing the super-hydrophobic coating on the surface of the substrate.
The coatings prepared in examples 1 to 4 and comparative example 1 were subjected to a performance test in which the contact angle test results are shown in table 1 and the scanning electron microscope test results are shown in fig. 1 to 2.
Contact angle test: using DSA30 type (Germany)
Company) contact angle measuring instrument measures the Contact Angle (CA) of a water drop on a coating film, the volume of the water drop is 10 μ L, the contact angle of 5 different points is measured for each sample, and the average value is finally taken.
And (3) testing by a scanning electron microscope: preparing a sample to be detected, scanning the sample under a scanning electron microscope SEM (FEI NANO SEM 450), and observing the micro appearance of the sample to be detected.
And (3) aging resistance test: an ultraviolet aging box is used for simulating an outdoor environment, the aging resistance of the super-hydrophobic coating is explored, the contact angle is tested once every 12 hours along with the irradiation of ultraviolet light, and when the contact angle is lower than 150 degrees, the test is finished.
Pencil hardness: various types of pencils are prepared, and the pencils are cut into cylindrical pencil cores with the length of about 4-6 mm. The pencil was held perpendicular to the sandpaper and rubbed on the sandpaper to obtain a flat-bottomed, sharp-edged pencil face. The pencil sample and the coating are pushed forward at a constant speed of 45 degrees.
From the test results of fig. 1, it can be seen that the sprayed colloidal suspension is solidified on the surface of the substrate to form a groove structure due to the phase separation of the crosslinked polymethylmethacrylate solution and the interpenetrating network of the polyurethane binder. It can further be seen from fig. 2 that with increasing magnification, fluorinated nanoparticles have been successfully embedded in the grooves, thereby improving the aging resistance.
Table 1 results of performance testing
| Sample (I) | Contact angle (degree) | Anti-aging time | Hardness of pencil |
| Example 1 | 166 | 48 hours | F |
| Example 2 | 164 | 72 hours | HB |
| Example 3 | 162 | 60 hours | H |
| Example 4 | 161 | 48 hours | 2H |
| Comparative example 1 | 160 | 24 hours | F |
As can be seen from Table 1, the superhydrophobic coatings prepared in examples 1-4 of the present application all have contact angles greater than 150 degrees and have superhydrophobic properties. And from the aging resistance time, the aging resistance time of the super-hydrophobic coating prepared in example 2 reaches 72 hours, and the aging resistance time is better. In addition, the super-hydrophobic coating prepared in example 2 has the lowest pencil hardness and the softest super-hydrophobic coating, so the wear resistance is better. Comparative example 1 had poor aging resistance due to the lack of fluorinated nanoparticles.
The super-hydrophobic coatings prepared in examples 1 and 5 to 7 were subjected to abrasion test, the super-hydrophobic coatings were rubbed with a rubber, the number of rubbing times was recorded, a contact angle test was performed every 5 cycles, and when the contact angle was less than 150 degrees, the test was terminated, and the test results are shown in table 2.
| Sample (I) | Number of wearing times |
| Example 1 | 80 times (twice) |
| Example 5 | 100 times (twice) |
| Example 6 | 80 times (twice) |
| Example 7 | 80 times (twice) |
As can be seen from Table 2, the abrasion times of the superhydrophobic coating prepared in example 5 reach 100 times, and it is known that the wear resistance of the superhydrophobic coating is better when the curing time of step (4) is 20 min.
It should be noted that the above-mentioned embodiments illustrate rather than limit the scope of the invention, and that those skilled in the art will be able to modify the invention in its various equivalent forms after reading the present invention and to fall within the scope of the invention as defined in the appended claims.
Claims (10)
1. A preparation method of a super-hydrophobic coating is characterized by comprising the following steps:
(1) adding ethyl acetate, methyl methacrylate, trimethylolpropane trimethacrylate and azobisisobutyronitrile into a reaction container to react to prepare a cross-linked polymethyl methacrylate solution;
(2) mixing the crosslinked polymethyl methacrylate solution with a polyurethane adhesive, and uniformly stirring to form a spray colloidal suspension;
(3) spraying the spray colloid suspension on the surface of the base material in a cold spraying mode, and curing at room temperature;
(4) and (4) on the basis of the step (3), spraying the fluorinated nano-particles on the surface of the base material in a cold spraying mode, and curing at room temperature to obtain the super-hydrophobic coating.
2. The method of preparing the superhydrophobic coating of claim 1, wherein in the step (1), 30-70 parts of the ethyl acetate, 10-50 parts of the methyl methacrylate, 5-40 parts of the trimethylolpropane trimethacrylate, and 1-20 parts of the azobisisobutyronitrile are added.
3. The method for preparing the superhydrophobic coating of claim 1, wherein the reaction temperature in the step (1) is 50-80 ℃.
4. The method for preparing the superhydrophobic coating of claim 1, wherein the reaction time in step (1) is 12-36 h.
5. The method for preparing a superhydrophobic coating according to claim 1, wherein in the step (1), the heating is performed by using an oil bath.
6. The method for preparing the superhydrophobic coating according to claim 1, wherein in the step (2), the addition amount of the cross-linked polymethyl methacrylate solution is 40-90% of the total amount of the cross-linked polymethyl methacrylate solution and the polyurethane binder; the adding amount of the polyurethane adhesive is 10-60% of the total amount of the crosslinked polymethyl methacrylate solution and the polyurethane adhesive.
7. The method for preparing the superhydrophobic coating of claim 1, wherein in the step (2), the mechanical stirring is performed for 1-4 hours.
8. The method for preparing the superhydrophobic coating according to claim 1, wherein in the step (3), the cold spraying is performed by using high-pressure gas from an air compressor.
9. The method of claim 1, wherein the fluorinated nanoparticles are selected from aluminum fluoride nanoparticles.
10. A superhydrophobic coating, prepared by the method of preparation of the superhydrophobic coating of any of claims 1-9.
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| CN202010881988.2A CN111974656A (en) | 2020-08-27 | 2020-08-27 | Super-hydrophobic coating and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112778808A (en) * | 2020-12-30 | 2021-05-11 | 嘉兴聚新航空材料科技有限公司 | Anti-icing super-hydrophobic coating for rotor wing of unmanned aerial vehicle |
| CN113172969A (en) * | 2021-04-26 | 2021-07-27 | 东莞市天桉硅胶科技有限公司 | Foaming silica gel cloth and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104910779A (en) * | 2015-06-04 | 2015-09-16 | 西安交通大学 | Super-hydrophobic acrylic polyurethane coating and preparation method thereof |
| CN106893454A (en) * | 2017-04-21 | 2017-06-27 | 黑龙江凯恩琪新材料科技有限公司 | A kind of preparation method of sprayable and durable super-amphiphobic coating |
-
2020
- 2020-08-27 CN CN202010881988.2A patent/CN111974656A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104910779A (en) * | 2015-06-04 | 2015-09-16 | 西安交通大学 | Super-hydrophobic acrylic polyurethane coating and preparation method thereof |
| CN106893454A (en) * | 2017-04-21 | 2017-06-27 | 黑龙江凯恩琪新材料科技有限公司 | A kind of preparation method of sprayable and durable super-amphiphobic coating |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112778808A (en) * | 2020-12-30 | 2021-05-11 | 嘉兴聚新航空材料科技有限公司 | Anti-icing super-hydrophobic coating for rotor wing of unmanned aerial vehicle |
| CN113172969A (en) * | 2021-04-26 | 2021-07-27 | 东莞市天桉硅胶科技有限公司 | Foaming silica gel cloth and preparation method thereof |
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Address after: 246000 south of Longshan East Road and west of Gaoqiao Road, Taihu Economic Development Zone, Anqing City, Anhui Province Applicant after: Anhui Fuyin New Materials Co.,Ltd. Address before: 246000 south of Longshan East Road and west of Gaoqiao Road, Taihu Economic Development Zone, Anqing City, Anhui Province Applicant before: Anhui Fuyin New Material Co.,Ltd. |
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Application publication date: 20201124 |